Water → HCID 66749849, 화합물

HRID 1893658노트

반응식

HRID 1893658 반응식
[NH2:1][CH:2]([C:6]([CH3:9])([CH3:8])[CH3:7])[C:3]([OH:5])=[O:4].O.[O:11]1[CH2:15][CH2:14][CH:13]([O:16][C:17](=O)[O:18]C2C=CC([N+]([O-])=O)=CC=2)[CH2:12]1.CCN(C(C)C)C(C)C>CC#N.CO>[CH3:7][C:6]([CH3:9])([CH3:8])[CH:2]([NH:1][C:17]([O:16][CH:13]1[CH2:14][CH2:15][O:11][CH2:12]1)=[O:18])[C:3]([OH:5])=[O:4]

참가 물질

7

반응물 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 3061312-Amino-3,3-dimethylbutanoic acidHCID 15343685HCID 15343685, 화합물

생성물 1

HCID 66749849HCID 66749849, 화합물수율 65%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6342Acetonitrile용매

실험 절차

2-Amino-3,3-dimethyl-butyric acid (551 mg, 4.2 mmol) was dissolved in CH3CN (15 mL), H2O (3 mL) and MeOH (3 mL). Carbonic acid 4-nitro-phenyl ester tetrahydro-furan-3-yl ester (1.6 g, 6.3 mmol) and DIEA (1.46 mL, 8.4 mmol) were added. This reaction mixture was allowed to stir at room temperature for 16 h. After concentrated, diluted with EtOAc, washed with brine and H2O, dried over Na2SO4, the crude product was purified on silica (12 g, 25-75% EtOAc/hexanes) to give intermediate 3,3-dimethyl-2-(tetrahydro-furan-3-yloxycarbonylamino)-butyric acid as a white solid (670 mg, 65%).

후처리

  1. concentrationAfter concentrated
  2. additiondiluted with EtOAc
  3. washwashed with brine and H2O
  4. dry with materialdried over Na2SO4
  5. customthe crude product was purified on silica (12 g, 25-75% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-d7579fbc2d31484799ddf52ffd4fcc1f
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08513186B2

반응 노트

불러오는 중…